Vaporizer



Sept. 3, 1963 A. B. BROERMAN VAPORIZER Filed Oct. 31, 1960 ".255 ew 5&5

mvzmoa A.B. BROERMAN M W ATTORNEYS United States Patent ware Filed Oct. 31, 1960, Ser. No. 66,131 3 Claims. (Cl. 122--32) This invention relates to a vaporizer. In one aspect it relates to an apparatus for vaporization of a liquid sample stream of at least two components for production of a vapor sample stream. In another aspect it relates to apparatus for vaporization of a liquid sample stream of at least two components for the continuous production of a vapor sample stream suitable for analysis in an analyzer requiring vaporous samples for analysis.

Chromatographic analyzers require that samples for analysis be in the vapor phase. This present apparatus for vaporization of liquid samples has special utility in the preparation of a liquid containing sample stream for use in a chromatographic analyzer.

An object of this invention is to provide a vaporization apparatus for the preparation of material for analysis in a chromatographic analyzer. Another object of this invention is to provide an apparatus for the vaporization of liquid samples containing at least two components for production of vapors suitable for analysis in a chromatographic analyzer. Still another object of this invention is to provide an apparatus for vaporizing a liquid sample stream containing at least two components of unequal boiling points for preparation of a vapor stream for analysis in an analyzer requiring vapor phase for analy- In the drawing, FIGURE 1 illustrates, in diagrammatic form and partly in section, apparatus suitable for carrying out the objects of this invention. FIGURE 2 is a section view taken on the line 22 of FIGURE 1. FIG- URE 3 is a vertical sectional view through the vaporizer vessel of FIGURE 1, taken on the line 3-3 of FIG- URE 2.

The vaporizing apparatus of this invention has particular utility in vaporizing such liquid streams as a mixture of butadiene and toluene, for example. Such a stream is found in an operation for production of cispolybutadiene synthetic elastomer.

In the drawing reference numeral 11 identifies a conduit communicating with a process point, not shown, through which liquid to be sampled is passing. A small fraction of the stream passing said process point is now passed through the conduit 11, through conduits 12 or 13 and through respective filters 14 or 15 for removal of foreign material so as not to plug up or interfere with subsequent operations. In this particular case, for example, the sample stream is passed through pipe 12 and filter 14 until such time as filter 14 needs replacing. At this time the valves in conduit 12 are closed and the valves in conduit 13 are opened and filter 15 is then on stream. Filter 14 is then replaced or cleaned. Fiitered liquid passes from the filters through a conduit 16, the flow being controlled by a flow controller apparatus 17. This flow controller apparatus is conventional in flow control art and broadly includes an orifice plate assembly, a motor valve and a controller instrument in which the rate of flow sensed by the orifice plate assembly is indicated or recorded in the controller and then a signal is emitted to a motor valve for opening or throttling same thereby increasing or decreasing the rate of flow of liquid as the case requires. The sample stream flows on through conduit 16, the pressure being regulated by a back pressure regulator 20. Pressure gauge 21 is inserted in conduit 16 for indication of pressure therein. However, if

3,102,512 Patented Sept. 3, 1963 "ice desired, this pressure gauge may be replaced by a recording pressure gauge in case a continuous record of pressure is desired. After passing through the back pressure regulator 20, the sample flows on through conduit 19 for such disposal as desired. A branch conduit 22 is connected with conduit 16 between the How controller 17 and the back pressure regulator 20. This conduit 22. is provided with a capillary tube 23. This capillary tube in one instance was a 3-inch long tube having a capillary diameter of 0.006 inch. This capillary tube is for the purpose of restricting flow of liquid through the conduit 22 so that a stream of relatively constant flow will enter subsequent apparatus.

The vaporizer proper comprises a vaporizer vessel assembly 24 provided with a dome-shaped bafile 27 sup ported by arms 28 attached to the inner surface of tank 24. The arms 28 are best seen in FIGURE 2. If desired, the arms 28 can be Welded to the inner surface of the wall of tank 25 or these arms may be fastened in any other suitable manner desired. This dome-shaped baflle 27 and supporting arms 28 are fixed in the vessel 25 at a location fairly near the top thereof. The upper portion of the vessel 25 is closed by a plate 42. Extend ing through the lower portion of the vessel is a standpipe 29, as illustrated. The lower end of this standpipe is closed while the upper end is open. A conduit 33 extends through the lower closed end of the standpipe and is provided with a back pressure regulator 36 for maintaining a suitable pressure in the tank or vessel 25. A conduit 35 is provided, as illustrated, for withdrawal of sample vapor for passage to an analyzer 37. Conduit 35 is intended to extend downward some little distance into the standpipe. 29 while the conduit 33 extends upward from the bottom of the standpipe a short distance as illustrated. The open and adjacent ends of the conduits 33 and 35 should be positioned some little distance from one another. A conduit 26 is wrapped around the outer surface of vessel 25 in the form of a coil for heating purposes. Steam is introduced into the coil through a conduit 31 and exits from the coil through a conduit 32. Conduit 32 is provided with a valve for regulation of the rate of flow of steam through the coil 26. When such a liquid material as a mixture of butadiene-toluene is vaporized in this vaporizer, provision is made by in stallation of a valved conduit 34 for removal of any polymer material formed during the vaporization. A very small amount of butadiene polymer tends to form because of the temperature required for the vaporization of the toluene. As illustrated in FIGURE 1, reference numeral 34 identifies a body of polymer in the bottom of vessel 25.

The analyzer 37 illustrated in FIGURE 1 is for this particular operation intended to be a chromatographic analyzer-recorder. A conduit 38 provides for passage of a carrier gas thereto while conduit 39 provides for venting of carrier gas and sample materials. When this analyzer is a recorder instrument, the process can be regulated by operation of, for example, a valve 41 in a process conduit 40.

When such a material as a butadiene-toluene mixture is being vaporized, after the sample emerges from the capillary tube 23 to an extension of conduit 22 of larger diameter than that of the capillary, some vaporization of the butadiene may occur. Also, since the tank 25 is heated by steam coil 26, the end of conduit 22 near the tank becomes heated and tends to assist in the vaporization of the sample before entry into the tank. This heating also tends to promote polymerization of the butadiene while at the same time any vaporization of the butadiene tends to cool the sample and thereby to restrict polymerization. The overall result is that little to no polymer 3 forms in the portion of conduit 22 nearest the vessel 25. However, since vaporization temperature has to be fairly high because of the high boiling point of the toluene in comparison to that of butadiene some polymer does form in the vaporization vessel 25. This polymer runs down the inner vessel walls and accumulates as a body of polymer 34 as illustrated. However, because of the rapid passage of sample material through the vessel 25 and the relatively short residence time therein, the rate of production of polymer is very, very small. Such an apparatus has been operated for several months at a time without need for withdrawal of polymer from the vaporizer vessel.

In the operation of the apparatus of this invention, a small stream of sample from a process point, not shown, passes through conduit 11 and through one or the other of filters 14 and 15 and thence through conduit 16. A small fraction of this sample stream is bypassed from conduit 16 through conduit 22 and through the capillary tube section 23. This bypassed material drops onto the upper surface of the dome-shaped bafile 27 at which point the butadiene easily vaporizes because of the temperature of the steam in the coils 26. The toluene is a little slower to evaporate but since the steam temperature is very near or slightly above the boiling point of the toluene, this latter material does evaporate quite rapidly. Since the back pressure regulator 36 is always open to some extent, there is a continuous flow of vapor through conduit 33 in such a manner that the vaporizer apparatus is a continuously operating vaporizer. Such an analyzer as a chromatographic analyzer 37 is operated in such a manner that its programmer withdraws samples at predetermined intervals for short periods of time from conduit 35. Thus, at any time that sample is withdrawn through conduit 35, the analyzer then determines and records the analysis of the sample.

A chromatographic analyzer-recorder-controller apparatus suitable for use with the sample vaporizer of this invention is fully described in US. Patent 2,875,606, in an application for patent, Serial No. 746,768, filed July 7, 1958. Still another chromatographic analyzer-recorder apparatus is described by Phillips Petroleum Company in ISA Journal, May 1960, page 76. Back pressure regulators suitable for use as regulator and regulator 36 are common instruments of the trade and are easily obtainable from instrument supply houses. Similarly, the flow controller 17 which can, if desired, be a flow recordercontroller is also a common apparatus and available from instrument supply houses.

A manually operable valve 18 is provided at the location illustrated in case the motor valve of the How controller 17 ever requires servicing.

As mentioned hereinabove, since some little vaporization of butadiene occurs in the portion of conduit 22 adjacent the vaporizer tank 25, there is little to no tendency for the formation of polymer in this section of conduit 22. Thus, this section of conduit 22 substantially never becomes plugged with polymer.

Materials of construction can be selected from those available in commerce taking into consideration any corrosive properties of the materials being vaporized.

Since the actual amount of vapor sample required for analysis in a chromatographic analyzer is not large, in one case, the volume of vessel 25 was approximately 300 cubic centimeters. Also, the inner diameter of the opening through the capillary tube 23 and its length can be selected to allow the proper rate of liquid flow therethrough taking into consideration the pressure maintained in conduit 16.

While certain embodiments of the invention have been described for illustrative purposes, the invention obviously is not limited thereto.

I claim:

1. A vessel for vaporizing a liquid in the production of the sample vapor representative of said liquid comprising, in combination, a closed vessel, said vessel having a longitudinal axis and being adapted to be positioned with its axis upright, a bafile rigidly mounted in said vessel, inlet means in said vessel for inlet of said liquid and being so positioned that said liquid drops from said inlet means onto said battle, a standpipe extending through the lower end of said vessel into said vessel, the outer end of said standpipe being closed and its inner end open, a first conduit extending from within said standpipe and from a level above the standpipe closed end but near thereto through said closed end to the exterior of said standpipe for outlet of vapor, an outlet for liquid in the end of said vessel adjacent said standpipe, a second conduit extending from within said standpipe and above said first conduit, through the wall of said vessel for outlet of vapor sample and means for heating said vessel.

2. A vessel for vaporizing a liquid in the production of a sample vapor representative of said liquid comprising, in combination, a closed vessel, said vessel having a longitudinal axis and being adapted to be positioned with its axis upright, a horizontally positioned baffle rigidly mounted in said vessel nearer its upper end than its lower end, inlet means in said vessel for inlet of a liquid containing fluid near said upper end in such a manner that said liquid drops onto said bafile, a standpipe extending through said other end into said vessel, the outer end of said standpipe being closed and its inner end open, a first conduit extending from within said standpipe and from a level above the standpipe closed end but near thereto through said closed end to the exterior of said standpipe for outlet of vapor, the space intermediate said standpipe and the vessel wall being a liquid accumulator, an outlet for liquid in the lower end of said accumulator, a second conduit extending from within said standpipe and above said first conduit through the wall of said vessel for outlet of vapor sample and means for heating said vessel.

3. A vessel for vaporizing a liquid in the production of a sample vapor representative of said liquid comprising, in combination, a closed vessel, said vessel having a longitudinal axis and being adapted to be positioned with its axis upright, a horizontally positioned bafile rigidly mounted in said vessel nearer its upper end than its lower end, inlet means in said vessel for inlet of a liquid containing fluid near said upper end in such a manner that said liquid drops onto said bafiie, said means including a capillary tube positioned therein in such a manner as to restrict flow of liquid through said inlet means, a standpipe extending through said other end in said vessel along its axis, the outer end of said standpipe being closed and its inner end open, a first conduit extending from within said standpipe and from a level above the standpipe closed end but near thereto through said closed end to the exterior of said standpipe for outlet of vapor, the space around said first conduit within said standpipe being a sump, an outlet for liquid in the lower end of said vessel adjacent said standpipe, the space intermediate said standpipe and the vessel wall being an accumulator, a second conduit extending from within said standpipe and above said first conduit through the wall of said vessel for outlet of vapor sample and means for heating said vessel.

References Cited in the file of this patent UNITED STATES PATENTS 1,439,206 Trumble Dec. 19, 1922 2,380,977 Lewis Aug. 7, 1945 2,452,143 Pellettere Oct. 26, 1948 2,777,428 Campbell et a1. Jan. 15, 1957 2,826,180 Lup'fer et al Mar. 11, 1958 

1. A VESSEL FOR VAPORIZING A LIQUID IN THE PRODUCTION OF THE SAMPLE VAPOR REPRESENTATIVE OF SAID LIQUID COMPRISING, IN COMBINATION, A CLOSED VESSEL, SAID VESSEL HAVING A LONGITUDINAL AXIS AND BEING ADAPTED TO BE POSITIONED WITH ITS AXIS UPRIGHT, A BAFFLE RIGIDLY MOUNTED IN SAID VESSEL, INLET MEANS IN SAID VESSEL FOR INLET OF SAID LIQUID AND BEING SO POSITIONED THAT SAID LIQUID DROPS FROM SAID INLET MEANS ONTO SAID BAFFLE, A STANDPIPE EXTENDING THROUGH THE LOWER END OF SAID VESSEL INTO SAID VESSEL, THE OUTER END OF SAID STANDPIPE BEING CLOSED AND ITS INNER END OPEN, A FIRST CONDUIT EXTENDING FROM WITHIN SAID STANDPIPE AND FROM A LEVEL ABOVE THE STANDPIPE CLOSED END BUT NEAR THERETO THROUGH SAID CLOSED END TO THE EXTERIOR OF SAID STANDPIPE FOR OUTLET OF VAPOR, AN OUTLET FOR LIQUID IN THE END OF SAID VESSEL ADJACENT SAID STANDPIPE, A SECOND CONDUIT EXTENDING FROM WITHIN SAID STANDPIPE AND ABOVE SAID FIRST CONDUIT, THROUGH THE WALL OF SAID VESSEL FOR OUTLET OF VAPOR SAMPLE AND MEANS FOR HEATING SAID VESSEL. 